CN106124436B - A kind of method that direct injected quickly measures lead content in dairy products - Google Patents
A kind of method that direct injected quickly measures lead content in dairy products Download PDFInfo
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- CN106124436B CN106124436B CN201610685619.XA CN201610685619A CN106124436B CN 106124436 B CN106124436 B CN 106124436B CN 201610685619 A CN201610685619 A CN 201610685619A CN 106124436 B CN106124436 B CN 106124436B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
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Abstract
The present invention is suitable for the technical field of food safety detection, disclose a kind of method that direct injected quickly measures lead content in dairy products, include the following steps: sample dilution, instrument parameter setting, production standard curve, sample solution measurement and standard curve standard measure, can quickly measure the lead content in dairy products.A kind of method that direct injected quickly measures lead content in dairy products of the present invention, it is measured using graphite furnace-Atomic Absorption Spectrometer with pyrolysis application type graphite-pipe, and the parameters such as the temperature of graphite furnace temperature program, time and gas flow are optimized according to the characteristic of sample solution, and it is not necessarily to sample pre-treatments, simple dissolved dilution only is carried out to sample, automatic sampling analysis can be applicable in, the simplification of sample handling procedure also reduces sample loss or contaminated possibility, interference is few, and accuracy improves.
Description
[technical field]
The present invention relates to the technical field of food safety detection, in particular to a kind of direct injected quickly measures in dairy products
The method of lead content.
[background technique]
With the rapid development of industry, metallic lead is used widely due to its special industrial application value.When various
Leaded industrial wastewater, exhaust gas are discharged into natural ecological environment, are caused serious pollution to soil and air, are gradually planted
Object and animal absorb, finally as the food in mankind's abdomen on food chain top.And lead and its compound respectively organize human body to have
Toxicity, route of intoxication can be sucked its steam or dust by respiratory tract, then in respiratory tract phagocyte by its rapid band to blood；
Or absorbed through alimentary canal, it is poisoned into blood circulation.Lead is by small intestinal absorption, and calcium, phytic acid and protein can hinder in diet
Hinder lead to absorb, cause acute poisoning, hemopoietic system damage, nervous system damage, kidney damage, immune system damage, to bone generation
Thank have an impact, have an impact to endocrine, genotoxicity, embryotoxicity, teratogenesis carcinogenesis.Therefore, lead content is carried out to food
Quantitative detection be necessary, and food lead content measuring method is complex at present, sample loss in detection process
Or contaminated possibility is larger, it is therefore necessary to propose a kind of method that direct injected quickly measures lead content in dairy products.
[summary of the invention]
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, a kind of direct injected is provided and quickly measures dairy products
The method of middle lead content aims to solve the problem that food lead content measuring method is complex in the prior art, sample in detection process
Loss or the larger technical problem of contaminated possibility.
To achieve the above object, the invention proposes a kind of method that direct injected quickly measures lead content in dairy products,
Include the following steps:
Step 1: sample dilutes: a certain amount of dairy products sample is accurately weighed in beaker, with a small amount of ultrapure water predissolve
Afterwards, it is transferred in 50mL volumetric flask, is settled to 50mL with ultrapure water, obtain sample solution, it is to be measured；
Step 2: instrument parameter is set: being configured to graphite furnace-Atomic Absorption Spectrometer optical parameter；
Step 3: production standard curve: being respectively 0,10.0ng/mL, 20.0ng/ with ultra-pure deionized water compound concentration
The lead standard solution of mL, 40.0ng/mL, 60.0ng/mL, 80.0ng/mL draw the lead mark of the above various concentration configured respectively
Quasi- each 10 μ L sample introduction of solution injects in graphite furnace-Atomic Absorption Spectrometer graphite-pipe, each concentration lead standard is measured after atomization
The absorbance value of solution, using absorbance value as ordinate, concentration is abscissa, and drafting obtains standard curve；
Step 4: sample solution measures: under test condition identical with lead standard solution, taking 10 μ L samples in step 1
Product solution sample introduction injects in graphite furnace-Atomic Absorption Spectrometer graphite-pipe, the absorbance of sample solution is measured after atomization
Value；
Step 5: standard curve standard measure: by the mark in the absorbance value and step 3 that measure sample solution in step 4
Directrix curve is compared quantitative lead content in the determining dairy products sample of finally calculating.
Preferably, the amount of weighing of the dairy products sample in the step one is 0.5g, weighs and is accurate to 0.0001g,
The ultrapure water is ultra-pure deionized water.
Preferably, beaker and volumetric flask in the step one are before being put into use, first through 20% nitric acid dousing, use
It after water repeated flushing, then is rinsed well with ultra-pure deionized water, is used after finally drying.
Preferably, the beaker and the volumetric flask soaking time in 20% nitric acid are greater than for 24 hours, the nitric acid is excellent
The pure nitric acid of grade.
Preferably, graphite furnace-Atomic Absorption Spectrometer graphite-pipe in the step two is using pyrolysis application type
Graphite-pipe, the optical parameter setting of the middle graphite furnace-Atomic Absorption Spectrometer are as follows: Detection wavelength 283.3nm, slit are wide
0.6nm, lamp current 6mA.
Preferably, graphite furnace-Atomic Absorption Spectrometer graphite furnace temperature program is divided into 8 stages, each
The temperature in stage, time heating method and gas flow are as shown in the table:
| Stage | Temperature (DEG C) | Time (s) | Heating method | Gas flow (L/min) |
| 1 | 105 | 10 | RAMP | 0.5 |
| 2 | 105 | 40 | STEP | 0.5 |
| 3 | 250 | 15 | RAMP | 0.5 |
| 4 | 600 | 10 | RAMP | 1 |
| 5 | 600 | 15 | STEP | 1 |
| 6 | 600 | 3 | STEP | 0 |
| 7 | 1800 | 2 | STEP | 0 |
| 8 | 2300 | 2 | STEP | 1 |
Preferably, in the step three each 10 μ L of the lead standard solution of various concentration sample introduction lead standard solution and step
10 μ L sample solution in rapid four, add 5 μ L matrix modifiers before sample introduction.
Preferably, the matrix modifier is ammonium dihydrogen phosphate or palladium nitrate solution.
Preferably, the concentration of the ammonium dihydrogen phosphate is 20.0g/L, the concentration of palladium nitrate solution is 50mg/
L。
Beneficial effects of the present invention: compared with prior art, a kind of direct injected provided by the invention quickly measures cream system
The method of lead content in product is measured using graphite furnace-Atomic Absorption Spectrometer with pyrolysis application type graphite-pipe, because cream is made
It is larger that product are dissolved in the dilution fluid viscosity obtained after water, and it is bad as a result, and therein that the temperature programming stage easily causes sample to splash etc.
Matrix composition is complicated, easily causes interference, therefore according to sample characteristics of for example to the temperature of graphite furnace temperature program, time and gas flow
Etc. parameters optimize, improve the accuracy of measurement, be not necessarily to sample pre-treatments, simple dissolved dilution only is carried out to sample, just
It can be applicable in automatic sampling analysis, the simplification of sample handling procedure also reduces sample loss or contaminated possibility, accuracy
Height, interference are few.
Feature and advantage of the invention will be described in detail by embodiment.
[specific embodiment]
In order to make the objectives, technical solutions and advantages of the present invention clearer, below by embodiment, to the present invention into
Row is further described.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
In limiting the scope of the invention.In addition, in the following description, descriptions of well-known structures and technologies are omitted, to avoid need not
Obscure idea of the invention in strategic point.
The embodiment of the present invention provides a kind of method that direct injected quickly measures lead content in dairy products, including walks as follows
It is rapid:
Step 1: sample dilutes: a certain amount of dairy products sample is accurately weighed in beaker, with a small amount of ultrapure water predissolve
Afterwards, it is transferred in 50mL volumetric flask, is settled to 50mL with ultrapure water, obtain sample solution, it is to be measured.
Specifically, the amount of weighing of dairy products sample is 0.5g, weighs and is accurate to 0.0001g, and ultrapure water is ultrapure deionization
Water.In the embodiment of the present invention, leaded steam or dust enter in sample solution in order to prevent, are preparing sample solution
Afterwards, it seals immediately, reduces interference.
Further, beaker and volumetric flask before being put into use, first through 20% nitric acid dousing, after water repeated flushing, then
It is rinsed well with ultra-pure deionized water, is used after finally drying.
Further, beaker and the volumetric flask soaking time in 20% nitric acid are greater than for 24 hours, and the nitric acid is excellent pure grade
Nitric acid.
Step 2: instrument parameter is set: being configured to graphite furnace-Atomic Absorption Spectrometer optical parameter.
Wherein, graphite furnace-Atomic Absorption Spectrometer graphite-pipe is using pyrolysis application type graphite-pipe, the middle graphite
Furnace-Atomic Absorption Spectrometer optical parameter setting are as follows: the wide 0.6nm of Detection wavelength 283.3nm, slit, lamp current 6mA.
Further, graphite furnace-Atomic Absorption Spectrometer graphite furnace temperature program is divided into 8 stages, each stage
Temperature, time heating method and gas flow are as shown in the table:
Step 3: production standard curve: being respectively 0,10.0ng/mL, 20.0ng/ with ultra-pure deionized water compound concentration
The lead standard solution of mL, 40.0ng/mL, 60.0ng/mL, 80.0ng/mL draw the lead mark of the above various concentration configured respectively
Quasi- each 10 μ L sample introduction of solution injects in graphite furnace-Atomic Absorption Spectrometer graphite-pipe, each concentration lead standard is measured after atomization
The absorbance value of solution, using absorbance value as ordinate, concentration is abscissa, and drafting obtains standard curve.
Specifically, the sample introduction lead standard solution of each 10 μ L of the lead standard solution of various concentration and 10 μ L samples in step 4
Solution adds 5 μ L matrix modifiers before sample introduction.
Further, matrix modifier is ammonium dihydrogen phosphate or palladium nitrate solution.
Further, the concentration of ammonium dihydrogen phosphate is 20.0g/L, and the concentration of palladium nitrate solution is 50mg/L.
Step 4: sample solution measures: under test condition identical with lead standard solution, taking 10 μ L samples in step 1
Product solution sample introduction injects in graphite furnace-Atomic Absorption Spectrometer graphite-pipe, the absorbance of sample solution is measured after atomization
Value.
Step 5: standard curve standard measure: by the mark in the absorbance value and step 3 that measure sample solution in step 4
Directrix curve is compared quantitative lead content in the determining dairy products sample of finally calculating.
In the concentration range of standard curve, the absorbance and concentration of lead element have good linear relationship, phase relation
Number is r >=0.999.Containing for lead element in dairy products can be quickly determined by dairy products sample solution lead element and linear formula
Amount.
The method that a kind of direct injected provided by the invention quickly measures lead content in dairy products is pyrolyzed application type using band
Graphite furnace-Atomic Absorption Spectrometer of graphite-pipe is measured, because of dairy products larger, the journey that is dissolved in the dilution fluid viscosity obtained after water
The sequence temperature rise period easily cause sample splash etc. it is bad as a result, and matrix composition therein it is complicated, easily cause interference, therefore according to sample
Product characteristic optimizes the parameters such as the temperature of graphite furnace temperature program, time and gas flow, improves the accuracy of measurement, nothing
Sample pre-treatments are needed, simple dissolved dilution only is carried out to sample, it will be able to it is applicable in automatic sampling analysis, sample handling procedure
Simplify and also reduce sample loss or contaminated possibility, interference is few, and accuracy improves.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (7)
1. a kind of method that direct injected quickly measures lead content in dairy products, characterized by the following steps:
Step 1: sample dilutes: a certain amount of dairy products sample is accurately weighed in beaker, after a small amount of ultrapure water predissolve,
It is transferred in 50mL volumetric flask, is settled to 50mL with ultrapure water, obtain sample solution, it is to be measured；
Step 2: instrument parameter is set: being configured to graphite furnace-Atomic Absorption Spectrometer optical parameter, wherein graphite
Furnace-Atomic Absorption Spectrometer graphite-pipe is using pyrolysis application type graphite-pipe, graphite furnace-Atomic Absorption Spectrometer optical parameter
Setting are as follows: the wide 0.6nm of Detection wavelength 283.3nm, slit, lamp current 6mA, graphite furnace-Atomic Absorption Spectrometer graphite furnace liter
Warm program is divided into 8 stages, and the temperature in each stage, time heating method and gas flow are as shown in the table:
Step 3: production standard curve: with ultra-pure deionized water compound concentration be respectively 0,10.0ng/mL, 20.0ng/mL,
The lead standard solution of 40.0ng/mL, 60.0ng/mL, 80.0ng/mL draw the lead standard of the above various concentration configured respectively
Each 10 μ L sample introduction of solution injects in graphite furnace-Atomic Absorption Spectrometer graphite-pipe, it is molten that each concentration lead standard is measured after atomization
The absorbance value of liquid, using absorbance value as ordinate, concentration is abscissa, and drafting obtains standard curve；
Step 4: sample solution measures: under test condition identical with lead standard solution, taking 10 μ L samples in step 1 molten
Liquid sample introduction injects in graphite furnace-Atomic Absorption Spectrometer graphite-pipe, the absorbance value of sample solution is measured after atomization；
Step 5: standard curve standard measure: the standard in the absorbance value and step 3 that measure sample solution in step 4 is bent
Line is compared quantitative lead content in the determining dairy products sample of finally calculating.
2. a kind of method that direct injected quickly measures lead content in dairy products as described in claim 1, it is characterised in that: institute
The amount of weighing of dairy products sample in the step of stating one is 0.5g, weighs and is accurate to 0.0001g, and the ultrapure water is ultrapure goes
Ionized water.
3. a kind of method that direct injected quickly measures lead content in dairy products as described in claim 1, it is characterised in that: institute
Beaker and volumetric flask in the step of stating one before being put into use, first through 20% nitric acid dousing, after water repeated flushing, then with super
Pure deionized water is rinsed well, is used after finally drying.
4. a kind of method that direct injected quickly measures lead content in dairy products as claimed in claim 3, it is characterised in that: institute
The beaker and volumetric flask stated soaking time in 20% nitric acid are greater than for 24 hours, and the nitric acid is excellent pure grade nitric acid.
5. a kind of method that direct injected quickly measures lead content in dairy products as described in claim 1, it is characterised in that: institute
The sample introduction lead standard solution of each 10 μ L of the lead standard solution of various concentration and 10 μ L samples in step 4 are molten in the step of stating three
Liquid adds 5 μ L matrix modifiers before sample introduction.
6. a kind of method that direct injected quickly measures lead content in dairy products as claimed in claim 5, it is characterised in that: institute
The matrix modifier stated is ammonium dihydrogen phosphate or palladium nitrate solution.
7. a kind of method that direct injected quickly measures lead content in dairy products as claimed in claim 6, it is characterised in that: institute
The concentration for the ammonium dihydrogen phosphate stated is 20.0g/L, and the concentration of palladium nitrate solution is 50mg/L.
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| CN107525777A (en) * | 2017-08-15 | 2017-12-29 | 东北制药集团股份有限公司 | A kind of method that lead content in amino acid injection-800 is detected using flame atomic absorption spectrometry |
| CN110118740A (en) * | 2019-06-26 | 2019-08-13 | 河南质量工程职业学院 | Measure the micro-wave digestion sampling Graphite Furnace Atomic Absorption analysis method of trace lead in white wine |
Citations (4)
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| CN103196849A (en) * | 2013-03-27 | 2013-07-10 | 广西中烟工业有限责任公司 | Detection method of lead content in triacetin |
| CN103499475A (en) * | 2013-09-26 | 2014-01-08 | 苏州国环环境检测有限公司 | Method of measuring lead content in shredded squid by microwave digestion-atomic absorption spectroscopy |
| CN104730010A (en) * | 2015-03-04 | 2015-06-24 | 嘉兴市产品质量检验检测院 | Method for detecting content of lead in zinc alloy button |
| CN105758812A (en) * | 2016-04-06 | 2016-07-13 | 云南新希望邓川蝶泉乳业有限公司 | Method for rapidly determining lead and chromium in dairy products |
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| JPH10318916A (en) * | 1997-05-14 | 1998-12-04 | Sumitomo Metal Mining Co Ltd | Determining method of nitrosyl ruthenium in tributyl phosphorate |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196849A (en) * | 2013-03-27 | 2013-07-10 | 广西中烟工业有限责任公司 | Detection method of lead content in triacetin |
| CN103499475A (en) * | 2013-09-26 | 2014-01-08 | 苏州国环环境检测有限公司 | Method of measuring lead content in shredded squid by microwave digestion-atomic absorption spectroscopy |
| CN104730010A (en) * | 2015-03-04 | 2015-06-24 | 嘉兴市产品质量检验检测院 | Method for detecting content of lead in zinc alloy button |
| CN105758812A (en) * | 2016-04-06 | 2016-07-13 | 云南新希望邓川蝶泉乳业有限公司 | Method for rapidly determining lead and chromium in dairy products |
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